US8578978B2 - Device for loading particles of catalyst into tubes having an annular zone - Google Patents

Device for loading particles of catalyst into tubes having an annular zone Download PDF

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Publication number
US8578978B2
US8578978B2 US12/896,444 US89644410A US8578978B2 US 8578978 B2 US8578978 B2 US 8578978B2 US 89644410 A US89644410 A US 89644410A US 8578978 B2 US8578978 B2 US 8578978B2
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United States
Prior art keywords
loading
tube
particles
annular zone
catalyst
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Expired - Fee Related, expires
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US12/896,444
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English (en)
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US20110083769A1 (en
Inventor
Elena Sanz
Robert Beaumont
Jérôme Colin
Fabrice Giroudiere
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IFP Energies Nouvelles IFPEN
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IFP Energies Nouvelles IFPEN
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Assigned to IFP Energies Nouvelles reassignment IFP Energies Nouvelles ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BEAUMONT, ROBERT, GIROUDIERE, FABRICE, Sanz, Elena, COLIN, JEROME
Assigned to IFP Energies Nouvelles reassignment IFP Energies Nouvelles CORRECTIVE ASSIGNMENT TO CORRECT THE INCORRECT APPLICATION NO. 12/869,999 AND DATE OF SIGNATURE OF 3RD INVENTOR PREVIOUSLY RECORDED ON REEL 025538 FRAME 0702. ASSIGNOR(S) HEREBY CONFIRMS THE DEVICE FOR LOADING PARTICLES OF CATALYST INTO TUBES HAVING AN ANNULAR ZONE. Assignors: COLIN, JEROME, BEAUMONT, ROBERT, GIROUDIERE, FABRICE, Sanz, Elena
Publication of US20110083769A1 publication Critical patent/US20110083769A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/003—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor in a downward flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/002—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor with a moving instrument
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00752—Feeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00769—Details of feeding or discharging
    • B01J2208/00778—Kinetic energy reducing devices in the flow channel

Definitions

  • the present invention relates to the field of devices that can be used to load catalyst present in the form of solid particles into multitubular reactors.
  • the particular nature of the loading medium concerned in the present invention is that it is constituted by the annular zone comprised between an outer tube and an inner tube.
  • the catalyst itself is constituted by particles that are generally cylindrical in shape, with a diameter of approximately 1 to 2 cm, and a length in the range 0.5 cm to 2 cm.
  • the present invention is not linked to a particular chemical reaction, but more generally concerns any reactor that uses bayonet tube type tube technology.
  • the reactors with which the present invention are concerned are large capacity natural gas steam reforming reactors for the production of synthesis gas (typically 100000 Nm 3 /h).
  • Such reactors are typically constituted by an assembly of approximately 200 to 300 tubes 15 meters in height enclosed in a shell that may reach 15 meters in diameter.
  • a major problem encountered in loading such multitubular reactors is that of homogeneity of the density of loading between the various catalytic tubes.
  • any heterogeneity in loading will result in a difference in the density of loading that may produce preferential passages from one tube to another, or even within the same tube. It is essential that the loading method employed ensures good homogeneity of density between the various catalytic tubes.
  • the loading method associated with the device must also be reproducible and sufficiently rapid so that the loading time remains within reasonable limits.
  • the prior art in the field of loading catalytic reactors is represented by two major types of loading, termed “dense” loading and “sock” loading.
  • the first of these loading techniques consists in distributing the particles of catalyst inside the reactor by causing said particles to rotate and to allow them to fall in the manner of raindrops.
  • That method results in dense, homogeneous loading but requires equipment for causing rotation that can distribute the catalyst over several radii in order to cover all of the catalytic section properly.
  • sock loading consists in introducing the particles of catalyst into the reactor through a flexible sock that is gradually lifted upwards as the level of particles of catalyst that are dispensed rises in the reactor. That method results in less dense loading than in “dense” loading, but the equipment is simpler.
  • the space available in the annular zone of a bayonet tube is typically of the order of 50 mm, i.e. about half that of a simple tube with a diameter of 100 mm.
  • the need to maintain the constancy of the annular space, i.e. good concentricity between the inner tube and the outer tube means that elements termed centralizers have to be installed between the outer tube and the inner tube, which centralizers are constituted, for example, by tabs fixed to one of the tubes, or tie rods connecting the walls of the inner and outer tubes.
  • said centralizers are 2 to 6 in number, and preferably 3 in number, over a given section.
  • said centralizers may be necessary to distribute these centralizers over 4 or 5 levels distributed in a regular manner along the tube.
  • angular sector will be used to designate the portion of space included between two consecutive centralizers.
  • the method of the present invention is a method that uses “grain-by-grain” loading and which necessitates a rigorous selection of the diameter of the loading tube with respect to the dimensions of the catalyst particles.
  • dmax denotes the largest dimension of a vat particle or grain
  • dmin denotes the smallest dimension of said particle
  • Dt must be both greater than 1.1 times dmax and less than 2 times dmin.
  • FIG. 1 is a diagrammatic view of a device in accordance with the present invention, showing the principal characteristics thereof;
  • FIG. 2 is a top view showing the angular sectors and the position of each sector of the loading tube
  • FIG. 3 is a diagrammatic view of the device of the present invention equipped with the optional system for extracting fine particles and braking the catalyst particles using a counter-current of gas.
  • the present invention can be defined as a device for loading particles of catalyst into the annular space of a bayonet type tube.
  • a bayonet tube is usually defined as being constituted by an outer tube with diameter Dext and an inner tube, concentric with the outer tube, with diameter Dint.
  • the annular space included between the outer tube and the inner tube constitutes the catalytic annular zone to be filled with particles of catalyst.
  • bayonet tubes are typically used in reactors for steam reforming various hydrocarbon feeds, especially natural gas; they are then in the form of a plurality of 200 to 300 tubes enclosed in a shell that may be up to 15 meters in diameter.
  • the device described in the present invention may be duplicated for the desired number of times in order to ensure simultaneous loading of several bayonet tubes.
  • the present invention is not linked to a particular shape of the catalyst particles.
  • the catalyst particles may have the form of small cylinders (7) that may possibly be perforated with small channels in order to increase the specific surface area of said particles.
  • the nub of the invention is the rigorous sizing of the loading tubes via which the catalyst particles are introduced into each of the sectors of the annular zone.
  • the diameter of the loading tubes must be just larger than the largest dimension of the catalyst particles while also being less than 2 times the smallest dimension of said particles.
  • the term “just larger” means a value of 1.1 times the largest dimension of the particles.
  • centralizers connect the inner wall of the outer tube and the outer wall of the inner tube.
  • Said centralizers are present in a number in the range 2 to 6 per section, preferably in a number of 3 per section of reaction tube.
  • Said centralizers are distributed along the bayonet tube and also contribute to its rigidity, which is an important aspect of good operability of the reactor.
  • the loading device of the present invention can thus allow loading of catalyst particles into the annular zone of a bayonet tube the annular section of which is divided into N angular sectors by elements termed centralizers, said device comprising:
  • length of the loading tube substantially equal to that of the bayonet tube means that the length of loading tube is less than that of the bayonet tube by less than 1 meter, and preferably by less than 0.5 meter.
  • the number of angular sectors is in the range 3 to 6; preferably, it is 3.
  • the device may be completed by a system for extracting fine particles.
  • the device may be completed by a system for braking particles intended to limit their velocity as they descend in the loading tube, generally disposed vertically or substantially vertically.
  • This system for braking catalyst particles may consist of cylindrical elements disposed perpendicular to the axis of said loading tube and fixed to the wall of said tube with a vertical spacing of 1 meter plus or minus 10 cm.
  • substantially vertical means that the bayonet tube (and thus the associated loading tube) makes an angle of plus or minus 30° with respect to the vertical.
  • the loading device of the invention can carry out loading at a homogeneous density over the entire length of the bayonet tubes as well as between the various bayonet tubes constituting the catalytic zone of the reactor.
  • the invention also pertains to the method for using the device that is described in the next paragraph.
  • the device for loading particles of catalyst into the annular zone of a bayonet tube comprises the following elements which are described in the order in which the catalyst particles advance.
  • the numbers refer to FIGS. 1 and 2 :
  • This set may be completed by a system for extracting fine particles of catalyst ( 10 , 12 in FIG. 3 ).
  • a braking system for said particles.
  • cylindrical elements of flexible material sort of “cilia” disposed perpendicular to the axis of said loading tube, denoted ( 9 ) in FIG. 1 , and fixed to the wall of said tube with a vertical spacing of approximately 1 meter, the spacing being variable as a function of the fragility of the catalyst to be loaded.
  • Another example of braking is the use of a rising stream of air created by aspiration ( 11 ), ( 12 ), or blowing the air (denoted ( 13 ), ( 14 ) in FIG. 3 ).
  • a filtration device 10
  • fine particles of catalyst means fragments of particles deriving from attrition, and which have a dimension of less than 1 mm.
  • the quality of loading is verified by measuring the pressure drop ( ⁇ P) of the catalytic bed filling the annular zone, i.e. between the inlet to the bayonet tube on the catalyst side (upper end of annular space) and the outlet from the bayonet tube (upper end of the inner tube).
  • the measurement of ⁇ P is carried out by causing a flow of air to pass through the tube loaded with catalyst.
  • Good loading corresponds to a deviation in ⁇ P between two tubes of less than ⁇ 5% with respect to the mean, which ensures a homogeneous distribution of particles of catalyst between the various tubes.
  • the method for loading a bayonet tube consists of the following series of steps:
  • the dimensions of the catalyst particles with a cylindrical shape were:
  • the loading device was constituted by:
  • Each loading tube was composed of an assembly of 11 ⁇ 1 meter sections.
  • the height of the fall is determined as the distance separating the upper end of the layer of particles already loaded into the annular zone and the outlet end of the loading tube.
  • Loading operation 1 2 3 4 Mass of loaded 189 187 187 183 grains (kg) Loading height 11850 11850 11850 (mm) Loading vol- 186 186 186 ume (liter) Bed density 1017 1003 1003 981 (kg/m 3 ) Air flow rate 70 70 70 (m 3 /h) ⁇ P (mbar) 183.2 177.7 180.3 171.2 Mean deviation +2.86% ⁇ 0.21% +1.22% ⁇ 3.87% of ⁇ P/mean ⁇ P
  • the loading time for one tube was approximately half an hour.
  • the total time for loading all of the 280 tubes was 35 hours, grouping the bayonet tubes in groups of 70. Four loading devices were used in parallel.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Catalysts (AREA)
US12/896,444 2009-10-01 2010-10-01 Device for loading particles of catalyst into tubes having an annular zone Expired - Fee Related US8578978B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR09/04.683 2009-10-01
FR0904683 2009-10-01
FR0904683A FR2950822B1 (fr) 2009-10-01 2009-10-01 Dispositif de chargement de particules de catalyseur dans des tubes presentant une zone annulaire

Publications (2)

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US20110083769A1 US20110083769A1 (en) 2011-04-14
US8578978B2 true US8578978B2 (en) 2013-11-12

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US (1) US8578978B2 (fr)
EP (1) EP2314371B1 (fr)
JP (1) JP5739128B2 (fr)
CN (1) CN102029127B (fr)
CA (1) CA2715915C (fr)
ES (1) ES2388815T3 (fr)
FR (1) FR2950822B1 (fr)
PL (1) PL2314371T3 (fr)
RU (1) RU2542282C2 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
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US20140290788A1 (en) * 2013-04-02 2014-10-02 Arkema France Method for filling a multitube catalytic reactor
US20150258518A1 (en) * 2012-10-17 2015-09-17 IFP Energies Nouvelles Pneumatic system for densely loading catalyst into bayonet tubes for a steam reforming reactor-exchanger with a detachable feed tube for gas
US20150298085A1 (en) * 2012-10-17 2015-10-22 IFP Energies Nouvelles Pneumatic system for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using an auxiliary tube for introducing solid particles
US9452400B2 (en) 2012-10-17 2016-09-27 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using removable deflectors
US9486764B2 (en) 2012-10-17 2016-11-08 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using removable helical elements
US9492802B2 (en) 2012-10-17 2016-11-15 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using flexible and removable slowing elements

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US8646492B2 (en) * 2010-05-24 2014-02-11 Extundo Incorporated Device for loading catalyst into a reactor vessel
US9149778B2 (en) 2010-05-24 2015-10-06 Extundo Incorporated Device and method for dispensing catalyst pellets
US9138709B2 (en) 2010-05-24 2015-09-22 Extundo Incorporated Device and method for dispensing pellets
CN103041753B (zh) * 2011-10-12 2015-04-01 中国石油化工集团公司 一种固定床反应器列管装填催化剂的加料装置及加料方法
CN104254391B (zh) 2012-04-23 2016-10-05 墨里克国际有限责任公司 催化剂加载工具
WO2013160310A1 (fr) * 2012-04-23 2013-10-31 Mourik International B.V. Dispositif de chargement de matériau particulaire
US20140037419A1 (en) * 2012-08-06 2014-02-06 Exxonmobil Research And Engineering Company Process for reactor catalyst loading
ES2621886T3 (es) * 2013-11-04 2017-07-05 Petroval Proceso para cargar material en partículas en un contenedor vertical estrecho
EP3015163B1 (fr) * 2014-10-31 2020-09-30 Petroval Procédé de chargement de particules en céramique dans un réacteur vertical
FR3033265B1 (fr) * 2015-03-04 2017-03-24 Ifp Energies Now Reacteur a lit incline permettant de mettre en œuvre de faibles quantites de catalyseur
AU2018255306B2 (en) * 2017-04-20 2022-09-08 Tubemaster, Inc. Method for loading pellets
CN107031875B (zh) * 2017-06-12 2019-02-19 南昌市豪尔科技印刷有限公司 一种火石包装机
US10576455B2 (en) 2018-03-22 2020-03-03 Air Products And Chemicals, Inc. Particle loading method and apparatus for a radial flow vessel
EP3542894A1 (fr) * 2018-03-22 2019-09-25 Air Products And Chemicals, Inc. Procédé et appareil de chargement de particules pour récipient à écoulement radial
WO2020203049A1 (fr) * 2019-03-29 2020-10-08 三菱ケミカル株式会社 Procédé de chargement de substance granulée
DK180737B1 (en) * 2020-07-06 2022-02-10 Marel Iceland Ehf A system and a method for automatically placing ice into boxes having two or more different widths
CN112660492B (zh) * 2020-12-09 2022-05-17 上海简逸生物科技有限公司 一种八连管适用的冻干微芯分装器
CN112623372B (zh) * 2021-01-07 2023-01-20 南京中隐客归网络科技有限公司 一种针对生物胶囊快速封装入盒设备
US20230112170A1 (en) * 2021-08-17 2023-04-13 Tubemaster, Inc. Device for loading pellets into reactor tubes

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US20150258518A1 (en) * 2012-10-17 2015-09-17 IFP Energies Nouvelles Pneumatic system for densely loading catalyst into bayonet tubes for a steam reforming reactor-exchanger with a detachable feed tube for gas
US20150298085A1 (en) * 2012-10-17 2015-10-22 IFP Energies Nouvelles Pneumatic system for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using an auxiliary tube for introducing solid particles
US9452400B2 (en) 2012-10-17 2016-09-27 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using removable deflectors
US9452399B2 (en) * 2012-10-17 2016-09-27 IFP Energies Nouvelles Pneumatic system for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using an auxiliary tube for introducing solid particles
US9486764B2 (en) 2012-10-17 2016-11-08 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using removable helical elements
US9486766B2 (en) * 2012-10-17 2016-11-08 IFP Energies Nouvelles Pneumatic system for densely loading catalyst into bayonet tubes for a steam reforming reactor-exchanger with a detachable feed tube for gas
US9492802B2 (en) 2012-10-17 2016-11-15 IFP Energies Nouvelles System for dense loading of catalyst into bayonet tubes for a steam reforming exchanger-reactor using flexible and removable slowing elements
US20140290788A1 (en) * 2013-04-02 2014-10-02 Arkema France Method for filling a multitube catalytic reactor
US9126166B2 (en) * 2013-04-02 2015-09-08 Arkema France Method for filling a multitube catalytic reactor

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EP2314371B1 (fr) 2012-05-30
JP5739128B2 (ja) 2015-06-24
CA2715915C (fr) 2016-05-31
EP2314371A1 (fr) 2011-04-27
RU2542282C2 (ru) 2015-02-20
JP2011072992A (ja) 2011-04-14
FR2950822A1 (fr) 2011-04-08
RU2010140147A (ru) 2012-04-10
CN102029127A (zh) 2011-04-27
FR2950822B1 (fr) 2012-02-24
CN102029127B (zh) 2014-10-29
CA2715915A1 (fr) 2011-04-01
ES2388815T3 (es) 2012-10-18
PL2314371T3 (pl) 2012-10-31
US20110083769A1 (en) 2011-04-14

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